Process of cleaning wool.



No. 63o,29s. Patented Aug. l, 1899.

,5. MAERTENS,

PROCESS 0F CLEANING WOOL.

(Application led June 24, 1899.)

(N u M o d el FROM rrILL..

STEAM /NVEN TUR.

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/ TNEESEE,

UNITED STATES PATENT' OFFICE.

EMILE MAER'TEN'S, OF PROVIDENCE, RHODE ISLAND.

eRoCl-:ss oF CLEANING WOOL..

sPE'cr'FrA''IoN forming part of Letters Patent No. 630,296, dated August 1, 1899.

i Application filed June 24, 1899. SerialNo. 721.733. (No specimens.)

T0 all .whom t may concern/ Be it known that I, EMILE MAERTENS, a citizen of the-United States, residingat Providence, in the county of Providence and State of Rhode Island, have invented certain new and useful improvements in the art of c l'eaning Wool and other animal fibers with volatile solvents, the object being to obtain the wool or liber in the best workable condition and to recover the by-products, such as wool-fat and the potash, of which the following is a specilication.

The invention relates more specifically to the process of removing the residual solvent lthe retention or condensation ofthe solvent gvapors contained in the air which is allowed A:to escape into the atmosphere, and may be which remains in the material under treatment after the fatty, oily, resinous, or other matters have been extracted therefrom, and is designed for use in establishments Where the output does not warrant the necessary expenditure for the more elaborate processes and apparatus described in my UnitedStates Patents Nos. 545,899, 545,900, and 615,030.

Referring to the accompanying drawings, Figure 1 is a general elevation of the apparatus with the digester shown in section. Fig.' 2 is a detail of the digester-cover, and Fig. 3 is a detail of the hydraulic plunger with its perforated extension or platen.

A is the digester, wherein the material to be extracted is placed, either while contained in a cage or basket or loose, and is supposed to be provided with suitable doors or covers for loading and unloading the material and closing the apparatus. It can also be of the special construction shown herein, which consist-s of the straight cylindrical part a, carrying at its top an enlarged annular chamber a', adapted. for the reception of a cover b and of heating-,coils c, and at its bottom a somewhat similar enlarged annularchamber 0.2,' adapted for the reception of heating-coils c and ot' a hydraulic ram d, having a Watertight packing at e. The cover b consists of the solid cap part b and of the foraminous hollow extension b2.

The ram d, which is shown Ain detail in Fig. 3, consists of the plunger d' (adapted to slide in the extension a3 ot chamber a2) and of the foraminous hollow extension or platen d2, which is fastened to it.

B is a reservoir provided with suitable heating-coils for the solvent used in the procgages, glasses, &c.

lconnected by suitable valved piping with all the other elements of the apparatus.

F is an oil condenser or extractor used for provided with heating means forfthe volatilization of the solvent retained by the oil in :said condenser.

G and lvl are drums or reservoirs provided with heating-coils and are adapted for the reception of liquids, for their separation, volatilization, or evaporation.

The various elements of the apparatus are provided wherever necessary with suitable valved inlet and outlet pipes, as well as with drain -cocks, thermometers, sight- The method for operating the apparatus is `as follows, the material' to be extracted or `treated being supposedly raw wool; The digester A having been charged with the wool `um is created in the digester A by putting the latter in communication with the pump 1E through valve l, pipes 100 and 101, and

valve 2. The air exhausted is discharged into the atmosphere through pipe 102 and valve 3. When a suitable vacuum has been obtained, the pump E is stopped and the valves previously opened are again closed. Steam' having been turned on to the coils in reservoirB by opening valve 4 on pipe 103 thepressure soon rises in this tank through the tension of the vapors of the solvent volatilized by the heat ot the coils, and when the internal pressure becomes sufficient valve 6 on pipe 104, valves 7, 8, and 9 on pi'pe 105, and valve 10 on IOO e l e,29

`or condenser C via pipe 107, valve 11, pipe 108, and valve 12 and from thecondenser'enters pipe 105 by Way of valve 13 on pipe 109 and valve 14 on pipe 110. When driving the solvent into pipe 105 by Way of the condenser C, valve 7 on pipe 105 must of course be closed.) The solvent containing extracted Wool-fat in solution from preceding opera-v tions is now forced from the bottom of the tank B through the pipes and valves j ust mentioned into the top of the digester A, which is filled therewith. Should a vacuum not have been made in the digester prior to the admission of the solvent, the latter is preferably allowed to enter at the bottom of the digester by valve 38, the airA displaced by the solvent being allowed to escape by opening valves 2 and 15 on pipe 101 and valve 16 on pipe 111 and enter the oil-condenserF through check-valve 17, where in passing through the oil contained therein it is stripped of the solvent vapors with which it is charged before escaping into the atmosphere through valve 18 on pipe 112, or it can first be passed through the condenser Gand from there to the condenser F by way of valves 19 and 20 on pipe 113, valve 21 on pipe 114, pipe 115, and valve 22 and check-valve 17 on pipe 111. The digester A being now fullof solvent containing wool-fat in solution, valve 6 cn pipe 104 is closed, valve 23 on pipe 116 is opened, and valve 7 on pipe 105 is closed.v The solvent vapors generated in reservoir B now rise through pipes 116 104 107, valve11, pipe 108,

and valve 12 and enter the condenser through pipe 114, from which they emerge in liquid form through pipe 109 and from there the pure solvent enters the top of digester A through valve 13, pipe 110, valve 14, pipe 105, valves 8,

Y 9, andlO, valve 38 being closed." Valve 24 on pipe 117 an'dvalve 25 on pipe 119 are now opened "and the charged solvent contained in digester A is allowed to return toA tank B through pipes 117, 118, and 119, care being taken by throttling valves 24 or 25 not to let the charged solvent from the bottom of digesterA into tank B any faster than the pure solvent from condenser Centers digester A at its top` and thus a complete continued immersion of the material being extracted is insured. If vdesired, the solvent from the digester can be run into drums H or G by opening valves 28 or 40 before beingv returned to tank B. When the whole of the material contained indigester A has'been suciently rinsed with the pure solvent coming from condenser C, valve 11on pipe 107 is closed, as well as valves 12 and 13 on the inlet and the outlet to the condenser C and valve 8 on pipe 105, whereas valve 7 on pipe 105, valve 26 on pipe 109, and valve 27 onv pipe 120 are opened, valve 14 on pipe 110 not having been closed. Meanwhile, all the liquid solvent contained in the digester Ahaving been drainedinto tank B, valve 25 on pipe 119 is closed. The vapors generatedin B now pass into the heater D, Where they are superheated, and from there through valve 10 into the top of the digester, or they can be sent direct from pipe 104 into pipe 105'thr0ugh valves 7, 8, 9, and 10 and be superheated in the chamber a by the coils` c. These superheated vapors, which are under pressure, somewhat compress the Whole mass of wool and at the same time heat it up to the point of vaporization of the residual solvent which it contains, and upon opening valve 28 'on pipe 121, leading into drum G, a quantity of liquid solvent kis `discharged into said drum, whereas vaporized solvent ascends pipe 122 into pipe 101 and from there enters the condenser by way ot' valve 15, pipe 113, valve 19, pipe 108, valve 12, and pipe 114 and when condensed is delivered into drum H or G via valve 29 on pipe 123 and valves 30 and 31. This operation is continued until substantially all the-residual solvent has been removed from the material. l have found by experience that the Wool is liable to be injured if in the treatment thereof the'temperature is allowed to go above 60 centigrade. Theexact temperature will vary with different wools,as Well i as with the nature of the solvent employed. The temperature which I prefer to employ in driving o the residual solvent from the wool is from 50o to 55 centigrade. Valves 4, 23, 9, and 28 are `now closed. Steam is turned on at valve 32 on pipe 106 for a few seconds, and this completely removes the last traces of solvent and deodorizes the'materiahwhich is now dry and degreased and in condition for removal from the digester in any suitable manner after atmosphericair'has been circulated through the material in orderto cool it off.

This is done by closing all lvalves previously opened, starting up thevacuum-pump, and

opening valve 3 on pipe 102, valve 1 on pipe 100, valve 2 on pipe 101, and valve 33 on pipe 124. This latter valve 33 admits atmospheric air,`which is drawn through the mass Yand discharged into the atmosphere either through valve 3 or by way of the oil-condenser F, via

valves 34 and 22 on pipe 115 and valve 18 on pipe 112, or by way of condenser C and the oil-condenser F, as previously described.

The removal of residual solvent bythe aid of superhe'ated solvent vapors alone is a tedious and dangerous operation, which unless carried on with great care and judgment is very liable to injure the material being treated when this is wool, and is notto be recom- 4mended even if ,carried on by very experi- IOO f tion with steam.

to pipe 106 by valve 32, Where it mixes with the solvent vapors before they enter the digester, the Water resulting from the condensation of the steam being separated from the solvent in drums H or G. 4

When the vacuum-pump is used with solvent vapors or With steam, or with both solvent vapors and steam, for the removal of the residual solvent, valve 28 on pipe 121, is closed, and all other valves being open or shut, as required, the vapors are circulated from the bottom of the digester through valve 24 on 117, through pipes 122 101 100, and through valve land are discharged by the pump E into condenser C, via pipe 102, valve 34, pipe 115, and valve 21 on pipe 114, the liqueed vapors finding theirway into drums H or G via pipe 109, valve 29, pipe 120, and valves 30 or 31.

Inlieu of solvent vapors 4Water-vapors are sometimes used for the removal of the residual solvent, and when this is the case valve 24 on pipe 117 is closed and the bottom chamber cof the digesteris filled or partially filled With Water by opening valves 35 and 36 on pipe 125. Steam is turned on to `coils c' of chamber 0.2 by opening valve 37. Valve 2 on pipe 101 and valve 1 on pipe 100 being opened and the vacuum-pump started, under the iniuence of the vacuum produced and the heat transmitted by coils c the water in chamber a2 is vaporized and drawn throughthe-contents of the digester, heating it up and vaporizing the residual solvent, which, along with the Water vapors, is delivered by the pump E into condenser C and from there into drums H or G, as previously described.-

In lieu of Water-vapors, of steam, of solvent vapors, or a combination of two'or three of the above, with or Without a vacuum, the residual solvent is sometimes removed by air, which is circulated over and over again through the material, preferably in con junc- When this is practiced, air is allowed to enter the system by valve 33 on pipe 124 or by any other inlet or inlets suitably situated for the purpose, and the pump E is started. If desired, the air may be indirectly heated prior to its introduction into the digester or may be directly heated by mixing steam therewith. The air is drawn through l the material and emerges from the digester through valve 2 on pipe 101, enters the pump through valve 1 on pipe 100, leaves the pump through pipe 102, enters the condenser through valve 34 on pipe 115 and valve 21 on pipe 114, passes through the condenser, leaving behind solvent and Water vapors which are condensed and run to tanks H or G via valve'29 on pipe 123 aud valves 30 or31, and through pipe 100 and valves 13 and 2G enters the heater D, Where it absorbs heat, emerges from the latter through pipe 120, enters pipe 105 through valve 27. and pipe 106 through valve 9L In pipe 106 it is preferably, mixed with steam injected through valve 32 and reenters the bottom chamber a2 of digester A through valve 38.

This air is thus circulated in a cycle, recooled, reheated,and remixed with steam until all ofthe residual solvent contain ed in the material held by the digester has been removed, and it is then discharged vinto the atmosphere by Way of the oil-condenser, as previously described.

In order to accelerate the removal of the residual solvent and before the circulation of steam, air, or vapors through the material, the latter can be squeezed for the expression of the bulk of the residual solvent. This is accomplished by making use of the ram d, (or of any equivalent device or 1neans,) which on being raised by the medium actuating it compresses the material betweenv the hollow foraminous platen d2 and the hollow foraminous extension b2 of the cover b, the liquid` expressed escaping through `the perforations of said platen and cover into chambers a' and a2 and emerging from there through valves 10 and 38 on pipe 106 .and valves 24 and 28 on pipe 117 and 121 into drum G. When the liquid has been expressed as described, the ram is again allowed to drop and the removalV of the still-adhering solvent is carried on as previously described.

1t is obvious that after treating the material and removing the cover b the digester can be emptied by the action of the plunger d', which when raised carries with it the holloW foraminous platen d2 and all that is supported' by the latter tothe top of the digester A, Where it is cared for in any suitable manner. Vhen the material being extracted is going to be subjectedto a subsequent Wet treatment in the digester itself, it is convenient to remove the residual solvent by means of the liquid or solution with which the material is to be treated or with Water, provided these are immiscible .with the` solventused in the extraction, and the operation is then as follows: Assuming that the liquid to be used is Water and that the material is to be partially prepared for carbonizing or entirely carbonized in the digester A and that the bulk of the residual solvent has or has not been removed by compression, as `described above, Water of a suitable temperature is allowed to enter digester A via valve 36, pipe 125, valve 35, and chamber d2. (it can, if need be, be heated by coils c' in said chamber) and to rise slowly in the part d, containing the extracted material. The adhering solvent is thereby nearly all removed and floated ou top of the Water or solution used. Vhen the floating solvent reaches chamber b2, the inlet flow of Water is reduced or stopped, steam is turned on the coil c by opening valve 39, and the floating solvent distilled off either in cacao, the vapors going through valves 2 and 1 and the pump on their Way to the condenser,

'or direct to the condenser via valve 2, pipe 101, valve 15, pipes 104 and 113, valve 19,

2, pipes 122 117, and valves 2S or 40.V Then lOO IIO

the solvent which has floated tothe top has n been removed, valve 2 is closed and the material is compressed by moving plunger d' upward, as previously described. This liberates further traces of solvent and also the natural soaps or potash salts con tained in the scribed, and the liquid containing the potash.

salts in solution is run into drums H or G by way of valves 10 and 38 on pipe 106 and valve 24., Apipe 117, and valves 28 or`40 for the re moval of traces of solvent, or it is run direct to a'st'orageetank by Way of valve 33 on pipe 124 for reuse or until its concentration warrants its vaporization for the recovery of the potash salts or other extracted material held in solution. The material can now after a slight steaming be removed from the digester and carried to the washers to be rinsed for the removal of extraneous impurities, or it can be further rinsed inthe digester itself by repeated immersions, compressions, and changes of water, and this is the case when it is desired to prepare the material for carbonizing or when it is desired to Vcarbonize` the material in the digester'itself or to remove it from the digester cleansed or cleansed and dried. Y

In order to prepare the material for carbonizingafter it has been sufficiently rinsed, it is j tinall'y compressed and the water allowed to drain out of the digester through valve 33 on pipe 124. The plunger d is then allowed to drop, and after closing valve 33 the carboniz'ing solution is introduced through valves 41 and 35 on pipe 125 `and chamber a2 into the part d of digester A. When` the material contained thereinls completely lmmersed by the solution, 'the flow is stopped and the material is allowed to steep for a suitable period. The solution is then allowed to return to its storage-tank through valve 33 on pipe A124 and the plunger d' is made to compress the material for the removal of the bulkV of the adhering carbonizing solution. The material can-now be removed to be dried, carbonized, neutralized, and redried, or it can be dried by passing steam and hot air through it in the manner previously described yand when dry carbonized by eliminating the steam from the circulation and increasing 'the temperature of the circulating air in the heater D and in coils c and c'. When the carbonization is complete, the material can be neutralized in the same manner that it was prepared for the carbonization by merely changing Vthe solution used. It v'can then be rinsed with water and after being pressed for the removal of the bulk of adhering moisture dried withhot air and steam, as previously described, when it Will be found in a nished and clean condition ready to be thrown out ofthe digester by operating the plunger d. The liquids accumulated in drums H and G are separated by decantation or evaporationg" for this purpose.

If desired, the material can be treated with water in the digester after the residual solvent has been removed by snperheated solventL vapors, water-vapors, air or steam, or both, or a combination of any of the means mentioned. If this water treatment is done thoroughly in the case of some wools, so as` vto remove all potash soaps present, and the wool is then partially dried, it can then in many cases be freely carded, and an expensive process can thus be saved. v

` When the solvent in tank B becomes too much saturated with extracted fat, apart of it is run to a still, where the fat is separated from the' solvent. The solvent is then returned to tank B by wayl of the condenser C direct or by way of condenser C and drums H and G in case the solvent is mixed wit-h water and needs separating in said drums.

Itis evident from the description and draw ings'that, if desired, the liquids, gases, or vapors used inthe process can beA passed through the digester in eitherdirection when it is deemed advisable or necessary to so do. It is evident that. the vacuum-pump can be dispensed with, if necessary, in some of the operations describedA and that the suction or vacuum created by the condensation of the vapors in the condenserwill to a great extent accomplish the same object.` Itis further evident that when the solvent used in the process is heavier than the extracted matter its flow throughther digester should be upward, whereas when the solvent is lighter than the extracted matter its tlow should be downward, and that in case of the lremoval of the residualsolvent with a liquid the flow of the liquid should be downward it the solvent is heavier than the liquid used for its removal, and that thetlow of said liquid should be upward through the digester .when the solvent is lighter than the liquid used for its removal. Y

The method hereinbefore described for removing residual solvent from wool by superheated solvent vapors is claimed in my application Serial No. 721,730.

The'described method ol removing residual solvent by the circulation of air in a closed vcircuit is claimed in my application Serial .then distilling 'od the solvent from the sur- IOO IIO

IIS

`face of the water, or aqueous solution, substantially as described.

2. The method of removing residual solvent from Wool which consists in removing the bulk of the residual solvent from the Wool by pressure, then floating the remainder of the solvent to the top of the vessel containing the Wool by the introduction of Water or aqueous solutions into the vessel, and then distilling oft' the solvent from the Water or aqueous solution, substantially as described.

3. The process of removing resid ual solvent from Wool and similar material which consists in carrying the same off by a current of Water and then separating it from the Water by distillation, substantially as described.

4. The method of removing residual solvent 'from Wool Which consists in removing the bulk of the residual solvent from the Wool by pressure, then floating the remainder of the solvent to the top of the vessel or precipitating vsaid solvent to the bottom of the vessel containing the` Wool, by the introduction of Water or aqueous solutions into said vessel and then separating the solvent from the Water or aqueous solutions, substantially as described.

5. The method of removing residual solvent from Wool which consists in introducing Water or aqueous solutions, hot or cold, into the digester containing the Wool, then eliminating the iioating solvent from the surface of the Water or aqueous solution or the precipitated solvent, from the bottom of the digester, then separating the bulk of the Water or aqueous solutions from the Wool, whereby the bulk of the potash or potash salts is also removed therefrom, substantially as described.

6. The method of removing residual solvent from Wool which consists in removing the bulk of the residual solvent from the Wool by pressure, then introducing Water or aqueous solutions, hot or cold, into the digester containing the wool, then eliminating the oating solvent from the surface of the Water or aqueous solutions or the precipitated solvent from the bottom of the digester, then separating the bulk of the Water or aqueous solutions from the Wool, whereby the bulk of the potash or potash salts is also removed therefrom, substantially as described.

7. The method of removing residual solvent from Wool which consists in oating the solvent to the top of the digester or precipitating it to the bottom of said digester, by the introduction of Water or aqueous solutions, then eliminating the solvent from the surface of the Water or aqueous solutions or from the bottom of the digester, then removing the potash or potash salts from the Wool and then steaming it, substantially as described.

S., The method of removing residual solvent from Wool Which consists in removing the bulk of the residual solvent from the Wool by pressure, then oating the solvent to the top ofthe digester or precipitating it to the bottornof said digester, bythe introduction of Water or aqueous solutions, then eliminating the solvent from the surface of the Water or aqueous solutions or from the bottom of the digester, then removing the potash or potash salts from the wool and then steaming it, substantially as described. r

9. The method of removing residual solvent from Wool which consists in separating the solvent from the Wool bythe introduction of Water or aqueous solutions, hot or cold, into the vessel containing the Wool, then separating the stratified solvent from the Water or aqueous solutions, then repassing Water or aqueous solutions through the Wool, substantially as described.

l0. The method of removing residual solvent from wool Which consists in floating said solvent above the Wool and to the top of the receptacle holding said Wool when the solvent used is lighter than Water and in precipitating said solvent to the bottom of the receptacle holding said Wool when the solvent used is heavier than Water, by means of a solution containing potash .salts which is passed through the Wool, and then separating the solvent from said solution, substantially as described.

EMILE MAERTENS.

Witnesses:

MABEL I. FAY, RUFUs S. MAT'rEsoN. 

